HRID40233

反应详情

EQUATION

反应方程式

HRID 40233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3,6-Dichloro-4-methylpyridazine (1.00 g, 6.1 mmol) was mostly dissolved in dioxane (22.5 mL) then added phenylboronic acid (0.82 g, 6.7 mmol), PdCl2(dppf)-CH2Cl2Adduct (0.25 g, 0.31 mmol) and a solution of cesium carbonate (6.0 g, 18 mmol) in water (7.5 mL). The reaction mixture was heated at 80° C. for 6 hours. The reaction mixture was concentrated under vacuum and the remaining solid was triturated with water. The solid was collected on a glass frit, washing well with water. The sample was purified by flash chromatography eluting with 1:4 ethyl acetate/hexane to afford 3-chloro-4-methyl-6-phenylpyridazine as an off-white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. customthe remaining solid was triturated with water
  3. customThe solid was collected on a glass frit
  4. washwashing well with water
  5. customThe sample was purified by flash chromatography
  6. washeluting with 1:4 ethyl acetate/hexane